KR101763427B1 - Process for producing antiglare antireflection film - Google Patents
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Abstract
The present invention relates to an adhesive sheet composition for a thin film solar cell, an adhesive sheet for a thin film solar cell using the same, and a thin film solar cell.
The present invention relates to a method for producing an antireflective antireflective film by spray-coating an antireflective composition comprising a fine particle and a solvent on a transparent base, wherein an antireflective layer is formed by the coated antireflective composition, Layer exhibits antistatic properties due to partial agglomeration of the fine particles contained in the antireflective composition, and the spray coating satisfies the conditions of the following formulas (1) and (2).
[Formula 1] F al = liquid amount (V) / (distance (D) * vapor pressure (P))
[Formula 2] 0.2 < F al < 0.7
(Unit: mm) of the antireflective composition ejected from the nozzle of the coater, and the distance D is a distance (unit: mm) between the nozzle and the transparent substrate, , And the vapor pressure (P) represents the vapor pressure (unit: mmHg) of the solvent contained in the antireflective composition.
According to the method for producing an antireflection film of the present invention, it is possible to produce a antireflection antireflection film having low reflection without any additional process by spray coating alone using an antireflection composition containing fine particles, It is possible to produce an antiglare antireflection film which does not deteriorate the performance of the antireflection film at the same time.
Description
The present invention relates to a process for producing an antireflection film, and more particularly, to a process for producing a antireflection film for antireflection used in an image display device such as a liquid crystal display device or a plasma display panel.
In a flat panel display device, a diaphragm antireflection film is required in order to improve visibility.
As an antireflection antireflection film, it is known to form an optical antireflection layer such as a low refractive index layer with a thickness of 50 to 200 nm on the surface of a antireflection film having a concavo-convex structure. The method of forming the antireflection layer on the surface of the antiglare layer having a concavo-convex structure by the vapor deposition method, the sputtering method, or the atmospheric pressure plasma film can form an antireflection layer having a uniform film thickness. However, It is not suitable for producing a uniformly large-area antiglare antireflection layer. On the other hand, there is proposed a manufacturing method of an antireflection antireflection layer by a coating method which is excellent in mass productivity, manufacturable at a reasonable cost, and suitable for producing a uniformly large antireflection antireflection layer.
However, when a low refractive index layer is applied to the surface of the concavities and convexities in accordance with the application method, leveling of the coating liquid lowers the irregularity of the concavities and convexities or uneven application occurs due to unevenness, And the film thickness is not uniform, so that the reflectance is not lowered as compared with the theoretical value, and there is a problem that color unevenness occurs due to the deviation of the film thickness.
In order to solve the above-mentioned problems, the present invention has been made to solve the above-mentioned problems, and it is an object of the present invention to provide an antireflective coating composition which is capable of forming a porous reflective layer by a spray coating method using conventional anti- And an object of the present invention is to provide a method for producing an antireflection film having antifogging properties.
In order to achieve the above object, the present invention provides a method for producing an antireflective antireflection film by spray-coating an antireflective composition comprising a fine particle and a solvent on a transparent substrate, And the reflection ring layer exhibits antistatic properties by partial agglomeration of the fine particles contained in the antireflective composition, and the spray coating satisfies the conditions of the
[Formula 1] F al = liquid amount (V) / (distance (D) * vapor pressure (P))
[Formula 2] 0.2 < F al < 0.7
(Unit: mm) of the antireflective composition ejected from the nozzle of the coater, and the distance D is a distance (unit: mm) between the nozzle and the transparent substrate, , And the vapor pressure (P) represents the vapor pressure (unit: mmHg) of the solvent contained in the antireflective composition.
In the method for producing an antireflective film according to the present invention, a hard coat layer may be formed on a transparent substrate, and then the antireflective composition may be spray coated thereon.
In the method for producing an antiglare antireflection film according to the present invention, the fine particles are preferably silica particles.
In order to achieve the above-mentioned other objects, the present invention provides the antireflective antireflection film produced by the process for producing a antireflective antireflective film according to the present invention.
According to the method for producing an antireflection film of the present invention, it is possible to produce a antireflection antireflection film having low reflection without any additional process by spray coating alone using an antireflection composition containing fine particles, It is possible to produce an antiglare antireflection film which does not deteriorate the performance of the antireflection film at the same time.
1 is a cross-sectional view of an antireflection type antireflection film according to an embodiment of the present invention.
2 is a cross-sectional view of the antireflection type antireflection film according to another embodiment of the present invention.
Hereinafter, the present invention will be described in more detail.
The present invention provides a method for producing an antireflective antireflective film by spray-coating an antireflective composition comprising fine particles and a solvent on a transparent substrate. In addition, the present invention provides a method for producing an antireflective antireflective film by forming a hard coat layer on the transparent substrate and then spray-coating the antireflective composition on the hard coat layer.
Each component constituting the antireflection film of the present invention will be described as follows.
Transparent substrate
Any transparent film may be used as the transparent substrate. For example, the transparent substance may be a cycloolefin-based derivative having a unit of a monomer including a cycloolefin such as norbornene or a polycyclic norbornene monomer, cellulose (diacetylcellulose, triacetylcellulose, acetylcellulose butyrate, iso Propyl cellulose, butyryl cellulose, acetyl propionyl cellulose), ethylene-vinyl acetate copolymer, polyester, polystyrene, polyamide, polyetherimide, polyacrylic, polyimide, polyethersulfone, polysulfone, There may be mentioned polyolefins such as polyethylene, polypropylene, polymethylpentene, polyvinyl chloride, polyvinylidene chloride, polyvinyl alcohol, polyvinyl acetal, polyether ketone, polyether ether ketone, polyether sulfone, polymethyl methacrylate, polyethylene terephthalate, poly Butylene terephthalate, poly It may be selected from selected from ethylene terephthalate, polycarbonate, polyurethane, epoxy, can be used an undrawn, uniaxially or biaxially stretched film. Preferably, uniaxial or biaxially stretched polyester films excellent in transparency and heat resistance, and triacetylcellulose films having no transparency and optically anisotropy can be used.
It is preferable that the transparent substrate is thin, but if it is too thin, the strength is lowered and the workability is poor. On the other hand, if it is too thick, transparency deteriorates or the weight of the polarizing plate becomes large. Therefore, the transparent substrate preferably has a thickness of about 8 to 1,000 탆, more preferably 40 to 100 탆.
Hard coating layer
The hard coat layer may be formed by a crosslinking reaction or a polymerization reaction of a photo-curable compound. Specifically, the hard coating layer can be formed by applying a hard coating composition comprising a photo-curable polyfunctional monomer or a polyfunctional oligomer on a transparent substrate, and crosslinking or polymerizing the polyfunctional monomer or polyfunctional oligomer.
The functional group of the photo-curable polyfunctional monomer or polyfunctional oligomer is preferably photo-polymerizable, electron-beam-polymerizable, or radiation-polymerizable. Of these, photopolymerizable functional groups are preferable. Examples of the photopolymerizable functional group include unsaturated polymerizable functional groups such as a (meth) acryloyl group, a vinyl group, a styryl group and an allyl group, and among them, a (meth) acryloyl group is preferable.
As the photopolymerizable compound, a compound having a radically polymerizable functional group such as a (meth) acrylate group, for example, a (meth) acrylate oligomer, a prepolymer or a monomer can be used.
Specific examples of the photopolymerizable multifunctional monomer having a photopolymerizable functional group include (meth) acrylates of alkylene glycols such as neopentyl glycol acrylate, 1,6-hexanediol (meth) acrylate and propylene glycol di (meth) Methacrylic acid diesters; (Meth) acrylate such as triethylene glycol di (meth) acrylate, dipropylene glycol di (meth) acrylate, polyethylene glycol di (meth) acrylate and polypropylene glycol di Esters; (Meth) acrylic acid diesters of polyhydric alcohols such as pentaerythritol di (meth) acrylate; Propylene oxide adducts such as 2,2-bis {4- (acryloxy diethoxy) phenyl} propane, 2-2-bis {4- (acryloxypolypropoxy) Methacrylic acid diester and the like. Also, epoxy (meth) acrylates, urethane (meth) acrylates, and polyester (meth) acrylates can be preferably used as photopolymerizable polyfunctional monomers.
Among the specific examples of the photopolymerizable polyfunctional monomer, esters of a polyhydric alcohol and (meth) acrylic acid are preferable. More preferably, a multifunctional monomer having three or more (meth) acryloyl groups in one molecule can be used. Specific examples thereof include trimethylolpropane tri (meth) acrylate, trimethylol ethane tri (meth) acrylate, 1,2,4-cyclohexanetetra (meth) acrylate, pentaglycerol triacrylate, pentaerythritol tetra (Meth) acrylate, dipentaerythritol tetra (meth) acrylate, dipentaerythritol hexa (meth) acrylate, dipentaerythritol triacrylate, dipentaerythritol pentaacrylate, dipentaerythritol tetra Erythritol triacrylate, tripentaerythritol hexatriacrylate, and the like. The multifunctional monomer may be used in combination of two or more.
Specific examples of the solvent include alcohols such as methanol, ethanol, isopropanol, butanol, methylcellulose, ethylsorbox and the like; ketones such as methyl ethyl ketone, methyl butyl ketone, methyl isobutyl ketone, diethyl ketone, , Hexane (hexane, heptane, octane etc.), benzene (benzene, toluene, xylene, etc.), and the like. The solvents exemplified above may be used alone or in combination of two or more thereof.
The solvent may be included in an amount of 30 to 80 parts by weight based on 100 parts by weight of the entire coating composition for forming an antireflective layer. If the amount of the solvent is less than 30 parts by weight, the coating is difficult because of high viscosity. If the amount of the solvent is more than 80 parts by weight, the curing process takes a long time and the cost is low.
For the polymerization reaction of the photopolymerizable multifunctional monomer, it is preferable to use a photoinitiator. As the photoinitiator, a photo radical initiator and a photo cation initiator are preferable, and a photo radical initiator is particularly preferable.
The photoinitiator may be used without limitation as long as it is used in the art. The photoinitiator specifically includes 2-methyl-1- [4- (methylthio) phenyl] 2-morpholinepropanone-1, diphenylketone benzyldimethylketal, 2- Dimethoxy-2-phenylacetophenone, anthraquinone, fluorene, triphenylamine, carbazole, 3-methylacetophenone, 4-chloroacetophenone, 4,4- 4,4-diaminobenzophenone, 1-hydroxycyclohexyl phenyl ketone, and the like. The above-exemplified photoinitiators may be used alone or in combination of two or more thereof.
When the photoinitiator comprises a hydrogen recycle type photoinitiator such as benzophenone, it is possible to improve the surface hardness by inhibiting the oxygen barrier effect, so that the photoinitiator may be a benzophenone based hydrogen recycle type photoinitiator.
Examples of the benzophenone type hydrogen recycling type photoinitiator include benzophenone, 2,4,6-trimethylbenzophenone, 4-methylbenzophenone, 4- (4-methylphenylthio) phenylmethanone, 3,3'- Benzoyl benzoate, methoxy benzophenone, methyl 2-benzoyl benzoate, 4-phenyl-benzophenone and 4,4'-bis (dimerylamino) -benzophenone. These may be used alone or in combination of two or more.
When a benzophenone-based hydrogen recycle type photoinitiator is used as the photoinitiator, a photosensitizer may be used together with the photoinitiator to minimize the problem of volatility generated during the photo polymerization and the oxygen problem.
Specific examples of the photosensitizer include amine (meth) acrylate or triethylamine, diethylamine, methyldiethanolamine, ethanolamine, isoamyl 4-dimethylaminobenzoate and the like. These may be used alone or in combination of two or more.
The photoinitiator may be included in an amount of 0.1 to 10 parts by weight based on 100 parts by weight of the coating composition for forming an antireflective layer. If the amount of the photoinitiator is less than 0.1 parts by weight based on the above-mentioned criteria, the curing rate is slowed. If the amount is more than 10 parts by weight, cracks may occur on the surface of the antireflection layer 120 due to over-curing.
In addition to the above-mentioned components, the hard coat composition used in the present invention may further include components commonly used in the art such as antistatic agents, antioxidants, UV absorbers, light stabilizers, thermal polymerization inhibitors, , A lubricant, an antifouling agent, and the like.
Antireflective composition
The antireflective composition of the present invention includes fine particles and a solvent, and may further include other additives.
The fine particles are added for the purpose of dispersibility, and it is preferable to use silica particles.
The silica particles are preferably spherical or amorphous, and spherical fine particles are more preferable for improving transparency. The surface of the silica particles is preferably treated with tetramethoxysilane to hydrophilically modify a hydrophilic hydroxy group in view of stability to a solvent.
The solvent may be used without limitation in the art. Specific examples of the solvent include alcohols (methanol, ethanol, isopropanol, butanol, methoxyethanol, methoxypropanol, etc.) or ketone solvents (methyl ethyl ketone, methyl butyl ketone, methyl isobutyl ketone, diethyl ketone, Etc.) can be preferably used.
These other additives may be used without limitation as long as they do not deviate from the object of the present invention and are generally used in the art. Specific examples of the other additives include an antioxidant, a UV absorber, a light stabilizer, a thermal polymerization inhibitor, a lubricant, a surfactant, and a lubricant.
BRIEF DESCRIPTION OF THE DRAWINGS Fig. 1 is a schematic cross-sectional view of an antireflective antireflection film according to the present invention. Fig. 2 shows that the antiglare
The
The coating thickness of the hard coating composition is 0.1 to 200 占 퐉, preferably 2 to 30 占 퐉, and more preferably 4 to 25 占 퐉. After the hard coating composition is applied, the volatiles are dried by evaporation at a temperature of 30 to 150 DEG C for 1 second to 30 minutes, preferably 10 seconds to 10 minutes. And then cured by irradiating UV light. The irradiation amount of the UV light is preferably about 0.01 to 10 J /
The thickness of the hard coat layer is not limited, but is preferably in the range of 1 to 30 mu m, more preferably in the range of 5 to 15 mu m.
The antiglare antireflection layer (2) is formed on the transparent substrate (1) by a spray coating method or on the hard coat layer (3) formed on the transparent substrate. As the spray coating method in the present invention, a conventional spray coating machine can be used.
When the antireflective antireflective coating layer is formed by the spray coating method, the antifogging property and the antireflective property can be controlled according to the type of solvent and the spraying conditions. The antireflective composition in the spray nozzle, that is, the fine particles of the coating liquid can be formed upon spraying the coating liquid, and a thin film can be formed.
Accordingly, in order to form an antireflective coating layer having antifogging property by coating once, according to the present invention, the following expression is derived through a process of controlling the agglomeration of particles by changing spray coating conditions according to the type of antireflective composition. Specifically, in order to confirm the antiglare antireflection performance according to the vapor pressure of the solvent of each parameter-antireflective composition, the amount of the antireflective composition ejected from the nozzle, and the distance between the nozzle and the transparent substrate in the present invention, .
[Formula 1] F al = liquid amount (V) / (distance (D) * vapor pressure (P))
(Unit: mm) of the antireflective composition ejected from the nozzle of the coater, and the distance D is a distance (unit: mm) between the nozzle and the transparent substrate, , And the vapor pressure (P) represents the vapor pressure (unit: mmHg) of the solvent contained in the antireflective composition.
Depending on the kind of the solvent contained in the antireflective composition, the state of the droplet until the droplet is ejected from the nozzle and reaches the substrate is changed. The higher the vapor pressure of the solvent, the faster the drying of the solvent in the droplets occurs during the spraying and the larger the aggregation of the particles occurs before reaching the substrate. On the other hand, when the vapor pressure of the solvent is low, drying of the solvent in the droplet occurs slowly, so that only the low refractive layer can be formed without agglomeration of the particles.
The state of the droplet can be controlled by controlling the distance between the spray nozzle and the substrate and the liquid amount of the coating liquid. The longer the distance between the nozzle and the substrate is, the longer the exposure time to the air is. Therefore, even if the solvent is the same, the solvent is further dried, and the agglomeration of the particles occurs and the haze increases. And was coated on the substrate to exhibit antireflection performance without aggregation. When the liquid amount of the coating solution is decreased, the size of the droplet becomes smaller.
In the spray coating process of the present invention, the antiglare and antireflective properties are controlled according to the respective conditions of the antireflective composition and the spray. The room was calculated F al factor as the expression and to determine the preferred conditions according to the distance to the overt liquid amount of the anti-reflection layer having a vapor pressure of a solvent used in the antireflective compositions used to produce the antireflective composition, the nozzle and the substrate. When the value of F al satisfies the following formula, excellent antiglare property and anti-reflection performance can be obtained in the present invention.
[Formula 2] 0.2 < F al < 0.7
Under the conditions of the spray coating used in the antiglare antireflection film of the present invention, the value of F al is greater than 0.2 and less than 0.7, as shown in the above equation. When the value of F al is less than 0.2, the haze is high and thus the anti-reflection property is greatly deteriorated. On the other hand, when the F al value is more than 0.7, the haze is low and good anti-reflection performance can be obtained. While having the anti-glare and anti-reflective property at the same time by selecting the F value in al the present invention in the above range it can be produced a room overt anti-reflection film that does not degrade the performance of each.
Hereinafter, the present invention will be described more specifically with reference to the following examples and comparative examples. The following examples are only illustrative examples of the present invention and are not intended to limit or limit the scope of protection of the present invention.
≪ Examples 1 to 5, Comparative Examples 1 to 4 >
- Preparation of Hard Coating Composition
40 parts by weight of pentaerythritol triacrylate (PE-3A), 0.5 part by weight of 1-hydroxycyclohexyl phenyl ketone (I-184, Ciba), 30 parts by weight of methyl ethyl ketone, 29.5 parts by weight of methyl isobutyl ketone Were added to prepare a composition.
- Preparation of antireflective composition
3 parts by weight of silica sol, and 97 parts by weight of methyl isobutyl ketone (vapor pressure: 14.8 mmHg) were mixed to prepare a composition.
≪ Examples 6 to 7 and Comparative Examples 5 to 6 >
- Preparation of Hard Coating Composition
40 parts by weight of pentaerythritol triacrylate (PE-3A), 0.5 part by weight of 1-hydroxycyclohexyl phenyl ketone (I-184, Ciba), 30 parts by weight of methyl ethyl ketone, 29.5 parts by weight of methyl isobutyl ketone Were added to prepare a composition.
- Preparation of antireflective composition
3 parts by weight of silica sol, and 97 parts by weight of the organic solvent described in Table 1 below were blended to prepare a composition.
- Manufacture of Antireflective Antireflection Film
Using the hard coating composition and antireflective composition prepared in Examples 1 to 7 and Comparative Examples 1 to 6, an antireflective antireflection film was prepared as follows. The above-prepared hard coating composition was bar-coated on a cellulose triacetate film (TAC) having a thickness of 80 탆 to form a coating layer. Then, the volatiles were evaporated at a temperature of 100 DEG C for 10 minutes, dried, and cured by irradiation with UV light of 2 J / cm < 2 >.
An antireflective coating liquid was coated on the formed hard coat layer using a spray coater under the conditions shown in Table 2 below. After forming an antireflective layer having antifogging properties, it was cured at 80 DEG C for 60 minutes.
(ml / min)
(mm)
(mmHg)
* Liquid amount: Liquid amount per hour of antireflective composition sprayed from the nozzle of the coater
** Distance: Distance between the nozzle of the coater and the transparent substrate
*** Vapor pressure: The vapor pressure of the solvent contained in the antireflective composition
<Test Example: Evaluation of Characteristics of Antireflection Antireflection Layer>
1) Reflectance
The manufactured antireflection film was adhered to a black acrylic plate using a pressure sensitive adhesive to remove the back reflection, and then the reflectance of the antireflection film was measured with a reflectance meter (UV-2450, manufactured by Shimadzu) to obtain the minimum reflectance. The results are shown in Table 3 below.
2) Hayes
The haze was measured using a haze meter (HZ-1, manufactured by Suga), and the results are shown in Table 3 below.
As a result of the above Table 3, it was confirmed that the antiglare performance and antireflection performance were controlled according to the liquid amount of the antireflective composition in the spray coating of the antireflective composition, the distance between the nozzle of the coater and the transparent substrate, and the vapor pressure of the solvent of the antireflective composition have. Specifically, it can be confirmed that when the F a1 value is larger than 0.2 and smaller than 0.7, it exhibits excellent antiglare performance and antireflection performance.
1: transparent substrate 2:
Claims (4)
An antireflection layer is formed by the coated antireflective composition and at the same time the antireflective composition exhibits antireflection properties by partial agglomeration of the particulates contained in the antireflective composition,
Wherein the spray coating satisfies the conditions of the following formulas (1) and (2).
[Formula 1] F al = liquid amount (V) / (distance (D) * vapor pressure (P))
[Formula 2] 0.2 < F al < 0.7
(Unit: mm) of the antireflective composition ejected from the nozzle of the coater, and the distance D is a distance (unit: mm) between the nozzle and the transparent substrate, , And the vapor pressure (P) represents the vapor pressure (unit: mmHg) of the solvent contained in the antireflective composition.
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| CN106054440B (en) * | 2016-07-25 | 2019-04-26 | 京东方科技集团股份有限公司 | A kind of array substrate and preparation method thereof and display device |
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